CN110203921A - A kind of preparation method of lithium ion battery modified natural graphite - Google Patents
A kind of preparation method of lithium ion battery modified natural graphite Download PDFInfo
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- CN110203921A CN110203921A CN201910508592.0A CN201910508592A CN110203921A CN 110203921 A CN110203921 A CN 110203921A CN 201910508592 A CN201910508592 A CN 201910508592A CN 110203921 A CN110203921 A CN 110203921A
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- lithium ion
- ion battery
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- flaky graphite
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 229910021382 natural graphite Inorganic materials 0.000 title claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 72
- 239000010439 graphite Substances 0.000 claims abstract description 67
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 63
- 239000002245 particle Substances 0.000 claims abstract description 53
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 238000010792 warming Methods 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 7
- 238000010348 incorporation Methods 0.000 claims description 8
- 238000012216 screening Methods 0.000 claims description 8
- 239000010426 asphalt Substances 0.000 claims description 5
- 125000002091 cationic group Chemical group 0.000 claims description 5
- 239000011339 hard pitch Substances 0.000 claims description 5
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 4
- 239000005011 phenolic resin Substances 0.000 claims description 4
- 229920001568 phenolic resin Polymers 0.000 claims description 4
- 229920001187 thermosetting polymer Polymers 0.000 claims description 4
- 239000011338 soft pitch Substances 0.000 claims description 2
- 229910021384 soft carbon Inorganic materials 0.000 abstract description 7
- 238000009792 diffusion process Methods 0.000 abstract description 5
- 239000003575 carbonaceous material Substances 0.000 abstract description 3
- 229910021385 hard carbon Inorganic materials 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 230000003014 reinforcing effect Effects 0.000 abstract description 3
- 240000003936 Plumbago auriculata Species 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 241000209456 Plumbago Species 0.000 description 3
- 238000005253 cladding Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of preparation methods of lithium ion battery modified natural graphite, comprising the following steps: (1) mixes flaky graphite particle with modified grain, modifying agent mass percent is 5%~30%；(2) step (1) resulting mixture is filled in container and is subsequently placed in carbide furnace, under nitrogen atmosphere or vacuum condition, the temperature in carbide furnace is warming up to 100~250 DEG C；(3) the resulting flaky graphite particle of step (2) is sent to vibromill, the sphericity of flaky graphite particle is adjusted by vibromill.In gap of the present invention by modifying agent being liquefied and being filled into natural spherical plumbago, structural stability after reinforcing spherical graphite roll-in, to enhance the liquid phase conduction of pole piece, enhance the high rate performance and cycle performance of pole piece, internal soft carbon and hard carbon material has biggish diffusion coefficient, the inside diffusion for being conducive to lithium ion, to enhance rapid charging performance.
Description
Technical field
The present invention relates to lithium ion battery negative material processing technique field, in particular to a kind of lithium ion battery is used
The preparation method of modified natural graphite.
Background technique
The natural spherical plumbago of lithium ion battery has a biggish cost advantage compared with artificial graphite, but there is compared with
The apparent disadvantages such as Cycle Difference and dynamic performance difference, since spherical graphite is to be made by natural flake graphite by spheroidization.
The prior art is usually that one layer of soft carbon is coated outside spherical natural graphite, and the method is relatively inaccessible to uniform cladding, is carbonized the day after tomorrow
Right graphite often more difficult compacting has apparent gap inside the spherical graphite that further nodularization is formed.Therefore, it is necessary to propose one
The new preparation method of kind, the gap of filled natural spherical graphite, the structural stability after reinforcing spherical graphite roll-in make spherical stone
More stable spherical morphology is able to maintain after ink roller pressure, when being applied to negative electrode of lithium ion battery, the inside for being conducive to lithium ion is expanded
It dissipates, to enhance rapid charging performance.
As it can be seen that the prior art could be improved and improve.
Summary of the invention
Place in view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of modified days of lithium ion battery
The preparation method of right graphite, it is intended to solve one layer of soft carbon of cladding outside spherical natural graphite in the prior art and be difficult to reach uniform packet
It covers and there is the technical issues of apparent gap in inside.
In order to achieve the above object, this invention takes following technical schemes:
A kind of preparation method of lithium ion battery modified natural graphite, which comprises the following steps:
(1) flaky graphite particle is mixed with modified grain, the modified grain is hard pitch, the drip of middle low temperature
Green, cationic emulsified bitumen or thermosetting phenolic resin；The modifying agent mass percent is 5%~30%；
(2) step (1) resulting mixture is filled in container and is subsequently placed in carbide furnace, in nitrogen atmosphere or vacuum
Under the conditions of, the temperature in carbide furnace is warming up to 100~250 DEG C；
(3) the resulting flaky graphite particle of step (2) is sent to vibromill, flaky graphite is adjusted by vibromill
The sphericity of grain.
Further, in the preparation method of the lithium ion battery modified natural graphite, in step (1), the squama
Exfoliated graphite particles are 100 mesh screenings.
Further, in the preparation method of the lithium ion battery modified natural graphite, flakey stone in step (1)
Black particle is mixed with modified grain by VC mixing machine；Incorporation time is 10~40 minutes.
Further, in the preparation method of the lithium ion battery modified natural graphite, VC is mixed in step (1)
The revolving speed of machine is 3~800r/min.
Further, in the preparation method of the lithium ion battery modified natural graphite, in step (2) with 3 DEG C/
The rate of min is warming up to 100~250 DEG C.
Further, in the preparation method of the lithium ion battery modified natural graphite, vibromill in step (3)
Spiral loading frequency is 1~5Hz, and host frequency is 20~70Hz, and grade frequency is 10~50Hz.
Further, in the preparation method of the lithium ion battery modified natural graphite, step passes through vibration in (3)
The sphericity of flaky graphite particle is adjusted to 70%~90% by mill.
The utility model has the advantages that the present invention provides a kind of preparation method of lithium ion battery modified natural graphite, compared to existing
Technology avoids in one layer of soft carbon of graphite particle external sheath in preparation method provided by the invention, but modifying agent is liquefied
And it is filled into the gap of natural spherical plumbago, the structural stability after reinforcing spherical graphite roll-in, after making spherical graphite roll-in
It is able to maintain more stable spherical morphology, to enhance the liquid phase conduction of pole piece, enhances the high rate performance and cycle performance of pole piece, it is interior
The soft carbon and hard carbon material in portion have biggish diffusion coefficient, are conducive to the inside diffusion of lithium ion, to enhance rapid charging performance.
Specific embodiment
The present invention provides a kind of preparation method of lithium ion battery modified natural graphite, to make the purpose of the present invention, skill
Art scheme and effect are clearer, clear, and the present invention is described in more detail by the following examples.It should be appreciated that this place
Specific examples are only used to explain the present invention for description, is not intended to limit the present invention.
The present invention provides a kind of preparation method of lithium ion battery modified natural graphite, method includes the following steps:
(1) flaky graphite particle is mixed with modified grain, the modified grain is hard pitch, the drip of middle low temperature
Green, cationic emulsified bitumen or thermosetting phenolic resin；The modifying agent mass percent is 5%~30%；
(2) step (1) resulting mixture is filled in container and is subsequently placed in carbide furnace, in nitrogen atmosphere or vacuum
Under the conditions of, the temperature in carbide furnace is warming up to 100~250 DEG C；
(3) the resulting flaky graphite particle of step (2) is sent to vibromill, flaky graphite is adjusted by vibromill
The sphericity of grain.
Among the above in step (1), the quality percentage of modifying agent refers to the original in flaky graphite particle and modifying agent composition
Mass percent shared by modifying agent in material.Described " hard pitch " its softening point be 150~250 DEG C, " middle soft pitch " its
Softening point is 50~150 DEG C.Wherein the effect of step (2) be make modified grain liquefaction be coated on natural flake graphite surface or
At dotted be adsorbed on crystalline flake graphite particle basal plane of liquefying.
Further, in step (1), the flaky graphite particle is 100 mesh screenings.
Further, flaky graphite particle is mixed with modified grain by VC mixing machine in step (1)；Incorporation time
It is 10~40 minutes.
Further, the revolving speed of VC mixing machine is 3~800r/min in step (1).
Further, 100~250 DEG C are warming up to the rate of 3 DEG C/min in step (2).
Further, the spiral loading frequency of vibromill is 1~5Hz in step (3), and host frequency is 20~70Hz, point
Grade frequency is 10~50Hz.
Further, the sphericity of flaky graphite particle is adjusted to 70%~90% by vibromill in step (3).
In order to make it easy to understand, further illustrating by the following examples.
Embodiment 1
The preparation method of the lithium ion battery modified natural graphite the following steps are included:
(1) flaky graphite particle is mixed with modified grain, the modified grain is middle low temperature temperature pitch；It is described
Modifying agent mass percent is 5%；The flaky graphite particle is 100 mesh screenings；Flaky graphite particle and modifying agent
Particle is mixed by VC mixing machine；Incorporation time is 10 minutes；The revolving speed of VC mixing machine is 3r/min；
(2) step (1) resulting mixture is filled in container and is subsequently placed in carbide furnace, in a nitrogen atmosphere, by carbon
The temperature changed in furnace is warming up to 100 DEG C with the rate of 3 DEG C/min；
(3) the resulting flaky graphite particle of step (2) being sent to vibromill, the spiral loading frequency of vibromill is 1Hz,
Host frequency is 20Hz, grade frequency 10Hz；Flaky graphite particle sphericity after vibromill is adjusted to 70%.
Embodiment 2
The preparation method of the lithium ion battery modified natural graphite the following steps are included:
(1) flaky graphite particle is mixed with modified grain, the modified grain is hard pitch；The modification
Agent mass percent is 25%；The flaky graphite particle is 100 mesh screenings；Flaky graphite particle and modified grain
It is mixed by VC mixing machine；Incorporation time is 20 minutes；The revolving speed of VC mixing machine is 100r/min；
(2) step (1) resulting mixture is filled in container and is subsequently placed in carbide furnace, under vacuum conditions, by carbon
The temperature changed in furnace is warming up to 250 DEG C with the rate of 3 DEG C/min；
(3) the resulting flaky graphite particle of step (2) being sent to vibromill, the spiral loading frequency of vibromill is 3Hz,
Host frequency is 50Hz, grade frequency 30Hz；The sphericity of flaky graphite particle is adjusted to 80%.
Embodiment 3
The preparation method of the lithium ion battery modified natural graphite the following steps are included:
(1) flaky graphite particle is mixed with modified grain, the modified grain is cationic emulsified bitumen；Institute
Stating modifying agent mass percent is 30%；The flaky graphite particle is 100 mesh screenings；Flaky graphite particle and modification
Agent particle is mixed by VC mixing machine；Incorporation time is 40 minutes；The revolving speed of VC mixing machine is 800r/min；
(2) step (1) resulting mixture is filled in container and is subsequently placed in carbide furnace, under vacuum conditions, by carbon
The temperature changed in furnace is warming up to 250 DEG C with the rate of 3 DEG C/min；
(3) the resulting flaky graphite particle of step (2) being sent to vibromill, the spiral loading frequency of vibromill is 5Hz,
Host frequency is 70Hz, grade frequency 50Hz；The sphericity of flaky graphite particle is adjusted to 90%.
Embodiment 4
The preparation method of the lithium ion battery modified natural graphite the following steps are included:
(1) flaky graphite particle is mixed with modified grain, the modified grain is thermosetting phenolic resin；Institute
Stating modifying agent mass percent is 25%；The flaky graphite particle is 100 mesh screenings；Flaky graphite particle and modification
Agent particle is mixed by VC mixing machine；Incorporation time is 30 minutes；The revolving speed of VC mixing machine is 600r/min；
(2) step (1) resulting mixture is filled in container and is subsequently placed in carbide furnace, in a nitrogen atmosphere, by carbon
The temperature changed in furnace is warming up to 100 DEG C with the rate of 3 DEG C/min；
(3) the resulting flaky graphite particle of step (2) being sent to vibromill, the spiral loading frequency of vibromill is 2Hz,
Host frequency is 50Hz, grade frequency 30Hz；The sphericity of flaky graphite particle is adjusted to 75%.
Embodiment 5
The preparation method of the lithium ion battery modified natural graphite the following steps are included:
(1) flaky graphite particle is mixed with modified grain, the modified grain is cationic emulsified bitumen；Institute
Stating modifying agent mass percent is 10%；The flaky graphite particle is 100 mesh screenings；Flaky graphite particle and modification
Agent particle is mixed by VC mixing machine；Incorporation time is 20 minutes；The revolving speed of VC mixing machine is 200r/min；
(2) step (1) resulting mixture is filled in container and is subsequently placed in carbide furnace, in a nitrogen atmosphere, by carbon
The temperature changed in furnace is warming up to 200 DEG C with the rate of 3 DEG C/min；
(3) the resulting flaky graphite particle of step (2) being sent to vibromill, the spiral loading frequency of vibromill is 3Hz,
Host frequency is 60Hz, grade frequency 30Hz；The sphericity of flaky graphite particle is adjusted to 82%.
Cathode of lithium battery is applied to the preparation-obtained flaky graphite particle of embodiment 1 to 5, and to 2C charging constant current
The projects such as section % (being charged as constant current constant voltage, blanking voltage 4.2V), button battery capacity, button battery first charge discharge efficiency are tested, and are surveyed
Test result is as follows:
By above-mentioned analysis it is found that compared with prior art, avoiding in preparation method provided by the invention in graphite particle
One layer of soft carbon of external sheath, but modifying agent is liquefied and is filled into the gap of natural spherical plumbago, reinforce spherical graphite roller
Structural stability after pressure is able to maintain more stable spherical morphology after making spherical graphite roll-in, so that the liquid phase for enhancing pole piece passes
It leads, enhances the high rate performance and cycle performance of pole piece, internal soft carbon and hard carbon material have biggish diffusion coefficient, be conducive to
The inside of lithium ion is spread, to enhance rapid charging performance.
It, can according to the technique and scheme of the present invention and its hair it is understood that for those of ordinary skills
Bright design is subject to equivalent substitution or change, and all these changes or replacement all should belong to protection scope of the present invention.
Claims (7)
1. a kind of preparation method of lithium ion battery modified natural graphite, which comprises the following steps:
(1) flaky graphite particle is mixed with modified grain, the modified grain be hard pitch, middle soft pitch,
Cationic emulsified bitumen or thermosetting phenolic resin；The modifying agent mass percent is 5%~30%；
(2) step (1) resulting mixture is filled in container and is subsequently placed in carbide furnace, in nitrogen atmosphere or vacuum condition
Under, the temperature in carbide furnace is warming up to 100~250 DEG C；
(3) the resulting flaky graphite particle of step (2) is sent to vibromill, flaky graphite particle is adjusted by vibromill
Sphericity.
2. the preparation method of lithium ion battery modified natural graphite according to claim 1, which is characterized in that step
(1) in, the flaky graphite particle is 100 mesh screenings.
3. the preparation method of lithium ion battery modified natural graphite according to claim 1, which is characterized in that step
(1) flaky graphite particle is mixed with modified grain by VC mixing machine in；Incorporation time is 10~40 minutes.
4. the preparation method of lithium ion battery modified natural graphite according to claim 3, which is characterized in that step
(1) revolving speed of VC mixing machine is 3~800r/min in.
5. the preparation method of lithium ion battery modified natural graphite according to claim 1, which is characterized in that step
(2) 100~250 DEG C are warming up to the rate of 3 DEG C/min in.
6. the preparation method of lithium ion battery modified natural graphite according to claim 1, which is characterized in that step
(3) the spiral loading frequency of vibromill is 1~5Hz in, and host frequency is 20~70Hz, and grade frequency is 10~50Hz.
7. the preparation method of lithium ion battery modified natural graphite according to claim 1, which is characterized in that step
(3) sphericity of flaky graphite particle is adjusted to 70%~90% by vibromill in.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110156005A (en) * | 2019-06-13 | 2019-08-23 | 广东凯金新能源科技股份有限公司 | A kind of preparation method of the graphite cathode material of fast charge lithium ion battery |
| CN111048785A (en) * | 2019-12-27 | 2020-04-21 | 深圳市金润能源材料有限公司 | Negative electrode material, preparation method thereof, electrode plate and battery |
| CN111463416A (en) * | 2020-04-14 | 2020-07-28 | 广东东岛新能源股份有限公司 | Low-cost low-expansion-rate long-circulation natural graphite-based composite material and preparation method and application thereof |
| CN119490183A (en) * | 2024-11-27 | 2025-02-21 | 宁波杉杉新材料科技有限公司 | Modified graphite material, preparation method, application and lithium ion battery |
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Application publication date: 20190906 |